CN115786025A - Organic urea calcium lithium lubricating grease and preparation method thereof - Google Patents

Organic urea calcium lithium lubricating grease and preparation method thereof Download PDF

Info

Publication number
CN115786025A
CN115786025A CN202211631497.8A CN202211631497A CN115786025A CN 115786025 A CN115786025 A CN 115786025A CN 202211631497 A CN202211631497 A CN 202211631497A CN 115786025 A CN115786025 A CN 115786025A
Authority
CN
China
Prior art keywords
calcium
lithium
grease
lubricating grease
organic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202211631497.8A
Other languages
Chinese (zh)
Other versions
CN115786025B (en
Inventor
程亚洲
汪利平
杨晓钧
褚铭铭
冯青姣
秦俊龙
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuxi PetroChina Lubricating Grease Co Ltd
Original Assignee
Wuxi PetroChina Lubricating Grease Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuxi PetroChina Lubricating Grease Co Ltd filed Critical Wuxi PetroChina Lubricating Grease Co Ltd
Priority to CN202211631497.8A priority Critical patent/CN115786025B/en
Publication of CN115786025A publication Critical patent/CN115786025A/en
Application granted granted Critical
Publication of CN115786025B publication Critical patent/CN115786025B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Lubricants (AREA)

Abstract

The invention discloses organic urea calcium lithium lubricating grease and a preparation method thereof, belonging to the technical field of general lubricating grease; the organic urea calcium lithium lubricating grease comprises the following components: base oil, isocyanate, organic amine, fatty acid, calcium hydroxide, lithium hydroxide, an antioxidant and an antirust agent. The organic urea calcium lithium lubricating grease has the advantages of high temperature resistance, long service life, strong water resistance and abrasion resistance, stronger universality, and lower raw material cost due to low lithium hydroxide consumption; by controlling the adding amount of the active organic amine and the reaction temperature, the method can effectively avoid the organic urea from wrapping other raw materials, realizes the production by one-step feeding and step-by-step reaction in the same reaction kettle, and also solves the problem of storage and hardening of the grease containing the calcium fatty acid.

Description

Organic urea calcium lithium lubricating grease and preparation method thereof
Technical Field
The invention relates to the technical field of universal lubricating grease, in particular to organic urea calcium lithium lubricating grease and a preparation method thereof.
Background
Among the general lubricating greases, the general lithium-based lubricating grease is the lubricating grease with the strongest universality and the largest market capacity at present, has the performance characteristics of good high temperature resistance, good shearing resistance, good water resistance, long lubricating life and the like, and is suitable for lubricating rolling bearings, sliding bearings and other friction parts of various mechanical equipment within the temperature range of-20 ℃ to 120 ℃. In recent years, the price of the main raw material lithium hydroxide of the universal lithium-based lubricating grease rises by more than ten times, and the supply of goods is very tight, so that great challenges are formed for enterprise production.
The production raw materials of the calcium-based lubricating grease and the polyurea lubricating grease do not need lithium hydroxide, and the production cost is obviously lower than that of the general lithium-based lubricating grease. The calcium-based lubricating grease has excellent water resistance and wear resistance, but has the problems of no high temperature resistance, poor shear resistance, short lubricating life, storage hardening and the like. The polyurea lubricating grease has excellent high temperature resistance, shear resistance and ultra-long lubricating life, but has the problems of poor water resistance and abrasion resistance. Therefore, the calcium-based grease and the polyurea grease cannot be called universal grease, and can be used instead of the universal lithium-based grease only under partial working conditions. If two or three of the calcium-based grease, the polyurea grease and the lithium-based grease are mixed in an appropriate ratio, the advantages are complemented with each other, and a universal grease can be obtained.
CN115247094A discloses a polyurea-anhydrous calcium-based lubricating grease and a preparation method thereof, wherein the polyurea lubricating grease and the anhydrous calcium-based lubricating grease are respectively prepared, and then the two lubricating greases are uniformly mixed, so that the performance of the prepared polyurea-anhydrous calcium-based lubricating grease is equivalent to that of the lithium-based lubricating grease.
CN102911773A discloses a composite calcium-lithium urea-based lubricating grease and a preparation method thereof, wherein the composite calcium-lithium urea-based lubricating grease prepared by introducing a calcium carboxylate salt into polyurea molecules has good adhesion, extreme pressure abrasion resistance and longer high-temperature bearing life.
CN112080328A discloses an organic lithium soap composite ureido grease and a preparation method thereof, wherein by introducing N-aminoethyl piperazine and an organic lithium compound, the extreme pressure anti-wear performance and the mechanical stability of grease are improved on the basis of keeping various original performances of the ureido grease unchanged.
CN1600843A discloses a preparation method of polyurea-lithium-based lubricating grease, organic amine and isocyanate are respectively melted in base oil, mixed and reacted, fatty acid is added after the reaction is finished, lithium hydroxide aqueous solution is added after the acid is melted for reaction, the temperature is raised to 190-220 ℃ after the reaction is finished, the temperature is kept, and the cooling and homogenization are carried out. The preparation method simplifies the preparation process and achieves the same effect as the prior art.
In the invention, one method is to prepare two lubricating greases respectively and then mix the two lubricating greases according to a certain proportion physically, the production operation is complex, and the other method is to carry out feeding reaction in multiple steps, so that the production operation is simplified, but a certain complexity still exists in the process of heating up, and the danger to feeding personnel can be increased newly. Only two kinds of lubricating grease are combined, the advantage complementarity may be insufficient, and the prepared lubricating grease has low universality. If the storage hardening problem cannot be solved after the introduction of the calcium-based grease, the universality of the grease is also limited, and the calcium-based grease cannot completely replace the general-purpose lithium-based grease.
Disclosure of Invention
In order to solve the technical problems, the invention provides the organic urea calcium lithium lubricating grease and the preparation method thereof, the organic urea calcium lithium lubricating grease has the advantages of high temperature resistance, long service life, strong water resistance and abrasion resistance, stronger universality, and lower raw material cost due to low lithium hydroxide consumption; by controlling the adding amount of the active organic amine and the reaction temperature, the method can effectively avoid the organic urea from wrapping other raw materials, realizes the production by one-step feeding and step-by-step reaction in the same reaction kettle, and also solves the problem of storage and hardening of the grease containing the calcium fatty acid.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
the organic urea calcium lithium lubricating grease comprises the following components in parts by weight: 70-90 parts of base oil, 0.5-5 parts of isocyanate, 0.5-5 parts of organic amine, 5-15 parts of fatty acid, 0.6-1.5 parts of calcium hydroxide, 0.1-1 part of lithium hydroxide, 0.1-0.5 part of antioxidant and 0.5-1 part of antirust agent.
Optionally, the base oil is at least one of mineral oil, synthetic ester base oil, and polyalphaolefin synthetic base oil; the kinematic viscosity of the base oil at 40 ℃ is 30-300 mm 2 /s。
Optionally, the fatty acid is at least one of dodecahydroxystearic acid, stearic acid, hydrogenated castor oil, and oleic acid.
Optionally, the calcium hydroxide is industrial grade calcium hydroxide or nano calcium hydroxide; the size of the calcium hydroxide particles is less than or equal to 74 mu m.
Optionally, the isocyanate is diphenylmethane-4, 4' -diisocyanate and/or 2, 4-toluene diisocyanate.
Optionally, the organic amine is at least one of cyclohexylamine, octadecylamine, dodecylamine, octylamine, p-toluidine and aniline.
Optionally, the antioxidant is at least one of diisooctyl diphenylamine, N-phenyl-a-naphthylamine, 2, 6-di-tert-butyl-p-cresol and 2, 6-di-tert-butyl-4-methylphenol.
Optionally, the rust inhibitor is at least one of benzotriazole, benzotriazole derivatives, thiadiazole derivatives, barium dinonylnaphthalenesulfonate, barium petroleum sulfonate, oxidized paraffin, and calcium lanolin soap or magnesium soap.
The embodiment of the invention also provides a preparation method of the organic urea calcium lithium lubricating grease, which comprises the following steps:
(1) Weighing the raw materials according to the weight part ratio of the raw materials of the organic urea calcium-lithium lubricating grease of any one of claims 1 to 8, putting two thirds of base oil, all isocyanate, organic amine, fatty acid, calcium hydroxide, lithium hydroxide and water into a reaction kettle, heating to 60-70 ℃, reacting for 0.5-1 h, heating to 100-110 ℃, reacting for 1-2 h, heating to 135-145 ℃, and refining and puffing for 0.5-1.5 h;
(2) Adding the remaining one third of the base oil to a quenching rotary kettle, standing for 24-48 h at 30-60 ℃, and starting the lubricating grease material to circulate for 0.5-1 h up and down every 8h of standing;
(3) And circularly shearing for 1-3 h by adopting a colloid mill, adding an antioxidant and an antirust agent, uniformly mixing, degassing and packaging to obtain the organic urea calcium lithium lubricating grease.
Compared with the prior art, the invention has the beneficial effects that:
(1) The organic urea calcium lithium lubricating grease integrates the polyurea lubricating grease, the calcium lubricating grease and the lithium lubricating grease through the process condition control, and combines the advantages of high temperature resistance and long service life of the polyurea lubricating grease and the advantages of strong water resistance and abrasion resistance of the calcium lubricating grease on the basis of the performance of the lithium lubricating grease. Compared with the general lithium-based lubricating grease, the organic urea calcium lithium lubricating grease has higher physical and chemical indexes and comprehensive performance and stronger universality, and simultaneously, the cost of raw materials is lower due to the low consumption of lithium hydroxide.
(2) Since isocyanate and organic amine usually react violently, the reaction product organic urea is formed quickly, and then if fatty acid, calcium hydroxide and lithium hydroxide raw materials are coated, the subsequent reaction is influenced. Therefore, the invention controls the adding amount of the active organic amine and the reaction temperature, controls the formation speed of the organic urea, can effectively avoid the organic urea from wrapping other raw materials, and realizes the production by one-step feeding and step-by-step reaction in the same reaction kettle.
(3) Since the calcium-based grease has a problem of storage hardening, the calcium-based grease prepared by reacting a small molecular acid with calcium hydroxide is hardened most severely, and secondly the long-chain fatty acid calcium-based grease also has a problem of slow storage hardening. At present, the hardening mechanism of the calcium-based lubricating grease is not clear, and researches show that high temperature, carbon dioxide and water are influencing factors of storage and hardening of the calcium-based lubricating grease, the carbon dioxide and the water can react with calcium hydroxide remained in the calcium-based lubricating grease to cause hardening of the lubricating grease, and the carbon dioxide and the water can change the morphological structure of fatty acid calcium to cause hardening of the lubricating grease. The organic urea calcium lithium lubricating grease refined after reaction is kept stand for 24-48 h under the controlled temperature, the lubricating grease material is started to circulate for 0.5-1 h every 8h of standing, the lubricating grease is contacted with carbon dioxide and trace water in the air, the lubricating grease can be hardened in a kettle, and the organic urea calcium lithium lubricating grease obtained is subjected to shearing treatment by a colloid mill, so that the hardening problem does not occur in the subsequent storage process.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The embodiment of the invention provides organic urea calcium lithium lubricating grease which comprises the following steps:
100kg of 500SN base oil, 2kg of diphenylmethane-4, 4' -diisocyanate ester, 1.2kg of cyclohexylamine, 0.88kg of octadecylamine, 16kg of dodecahydroxystearic acid, 1.95kg of calcium hydroxide, 0.32kg of lithium hydroxide and 2kg of water are put into a reaction kettle; heating to 65 ℃ and reacting for 1h; continuously heating to 110 ℃ and reacting for 1h; finally, heating to 140 ℃, refining and puffing for 1h; adding 50kg of base oil to a quenching rotary kettle, standing at 50 ℃ for 24 hours, and starting lubricating grease material to circulate up and down for 0.5 hour every 8 hours of standing; and circularly shearing for 3 hours by adopting a colloid mill, adding 0.5kg of diisooctyldiphenylamine and 1.2kg of barium dinonylnaphthalene sulfonate, uniformly mixing, and degassing to obtain the organic urea calcium lithium lubricating grease.
Example 2
The embodiment of the invention provides organic urea calcium lithium lubricating grease which comprises the following steps:
100kg of PAO10 base oil, 2.2kg of diphenylmethane-4, 4' -diisocyanate, 1.32kg of cyclohexylamine, 0.97kg of octadecylamine, 17.6kg of dodecahydroxystearic acid, 2.15kg of calcium hydroxide, 0.36kg of lithium hydroxide and 2kg of water are put into a reaction kettle; heating to 70 ℃ to react for 1h; continuously heating to 100-110 ℃ and reacting for 1h; finally, heating to 145 ℃, refining and puffing for 1h; adding 50kg of base oil into the quenching rotary kettle, standing for 48 hours at 60 ℃, and starting the lubricating grease material to circulate for 0.5 hour every 8 hours of standing; and (3) circularly shearing for 2 hours by adopting a colloid mill, adding 0.52kg of diisooctyldiphenylamine and 1.22kg of barium dinonylnaphthalenesulfonate, uniformly mixing, and degassing to obtain the organic urea calcium lithium lubricating grease.
Example 3
The embodiment of the invention provides organic urea calcium lithium lubricating grease which comprises the following steps:
100kg of 500SN base oil and 2.42kg of diphenylmethane-4, 4' -diisocyanate, 1.45kg of cyclohexylamine, 1.06kg of octadecylamine, 14.4kg of dodecahydroxystearic acid, 1.76kg of calcium hydroxide, 0.3kg of lithium hydroxide and 2kg of water are put into a reaction kettle; heating to 60 ℃ to react for 1h; continuously heating to 100 ℃ and reacting for 1h; finally, heating to 135 ℃ for refining and puffing for 1h; adding 50kg of base oil, rapidly cooling, transferring to a kettle, standing at 30-60 deg.C for 24h, and starting lubricating grease material to circulate for 0.5h every 8 h; and circularly shearing for 2.5 hours by adopting a colloid mill, adding 0.5kg of diisooctyldiphenylamine and 1.2kg of barium dinonylnaphthalene sulfonate, uniformly mixing, and degassing to obtain the organic urea-calcium-lithium lubricating grease.
Comparative example 1
The same as in example 1, except that the standing at 50 ℃ for 24 hours was cancelled and the grease mass was opened for 0.5 hour up and down cycles every 8 hours of standing.
Comparative example 2
The polyurea lubricating grease and the calcium-based lubricating grease are respectively prepared by taking 500SN as base oil, and then the polyurea lubricating grease and the calcium-based lubricating grease are physically mixed according to the proportion of 2 to 8 to prepare the product.
Comparative example 3
Commercially available general lithium grease of a certain brand.
Example of detection
The organic urea calcium lithium grease prepared in each example and comparative example is subjected to related performance tests, and the specific test results are shown in table 1 below.
TABLE 1 test results of performance of the organourea calcium lithium greases prepared in the examples and comparative examples
Figure BDA0004005848860000061
Figure BDA0004005848860000071
As can be seen from Table 1, the organic urea calcium lithium lubricating grease of the invention has good high temperature resistance, shear resistance, water resistance and long lubricating life, is not hardened during storage, and has comprehensive performance superior to that of certain brand universal lithium lubricating grease of comparative example 3.
The hardness of the 0-taper reaction grease in table 1 is smaller, the harder the grease is, and it can be seen from the data in the table that the 0-taper reaction grease is not substantially changed and the grease is not hardened after the products prepared in examples 1, 2 and 3 are stored at 40 ℃ for 7 days. The penetration at 0 times of the products prepared in the comparative examples 1 and 2 is obviously reduced after 7 days of storage at 40 ℃, and the lubricating grease has a hardening problem.
The product of example 1 was compared with the product of comparative example 2 in data, and the bearing lubrication life of example 1 was longer.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (9)

1. The organic urea calcium lithium lubricating grease is characterized by comprising the following components in parts by weight: 70-90 parts of base oil, 0.5-5 parts of isocyanate, 0.5-5 parts of organic amine, 5-15 parts of fatty acid, 0.6-1.5 parts of calcium hydroxide, 0.1-1 part of lithium hydroxide, 0.1-0.5 part of antioxidant and 0.5-1 part of antirust agent.
2. The organic urea calcium-lithium grease of claim 1 wherein the base oil is at least one of mineral oil, synthetic ester base oil, polyalphaolefin synthetic base oil; the kinematic viscosity of the base oil at 40 ℃ is 30-300 mm 2 /s。
3. The organic urea calcium-lithium grease of claim 1 wherein the fatty acid is at least one of dodecahydroxystearic acid, stearic acid, hydrogenated castor oil, oleic acid.
4. The organic urea calcium lithium grease of claim 1 wherein the calcium hydroxide is technical grade calcium hydroxide or nano calcium hydroxide; the size of the calcium hydroxide particles is less than or equal to 74 mu m.
5. The lithium calcium organourea grease according to claim 1 wherein the isocyanate is diphenylmethane-4, 4' -diisocyanate and/or 2, 4-toluene diisocyanate.
6. The grease of claim 1 wherein the organic amine is at least one of cyclohexylamine, octadecylamine, dodecylamine, octylamine, p-toluidine, and aniline.
7. The grease of claim 1 wherein the antioxidant is at least one of diisooctyldiphenylamine, N-phenyl-a-naphthylamine, 2, 6-di-t-butyl-p-cresol, 2, 6-di-t-butyl-4-methylphenol.
8. The organic urea calcium-lithium grease as claimed in claim 1, wherein the rust inhibitor is at least one of benzotriazole, benzotriazole derivatives, thiadiazole derivatives, barium dinonylnaphthalene sulfonate, barium petroleum sulfonate, oxidized paraffin, and calcium lanolin soap or magnesium soap.
9. A method of preparing an organourea calcium lithium grease according to any of claims 1 to 8 comprising the steps of:
(1) Weighing the raw materials according to any one of claims 1 to 8, adding two thirds of base oil, all isocyanate, organic amine, fatty acid, calcium hydroxide, lithium hydroxide and water into a reaction kettle, heating to 60-70 ℃, reacting for 0.5-1 h, heating to 100-110 ℃, reacting for 1-2 h, heating to 135-145 ℃, refining and puffing for 0.5-1.5 h;
(2) Adding the remaining one third of the base oil to a quenching rotary kettle, standing for 24-48 h at 30-60 ℃, and starting the lubricating grease material to circulate for 0.5-1 h up and down every 8h of standing;
(3) And circularly shearing for 1-3 h by adopting a colloid mill, adding an antioxidant and an antirust agent, uniformly mixing, degassing and packaging to obtain the organic urea calcium lithium lubricating grease.
CN202211631497.8A 2022-12-19 2022-12-19 Organic urea calcium lithium lubricating grease and preparation method thereof Active CN115786025B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211631497.8A CN115786025B (en) 2022-12-19 2022-12-19 Organic urea calcium lithium lubricating grease and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211631497.8A CN115786025B (en) 2022-12-19 2022-12-19 Organic urea calcium lithium lubricating grease and preparation method thereof

Publications (2)

Publication Number Publication Date
CN115786025A true CN115786025A (en) 2023-03-14
CN115786025B CN115786025B (en) 2024-04-12

Family

ID=85425730

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202211631497.8A Active CN115786025B (en) 2022-12-19 2022-12-19 Organic urea calcium lithium lubricating grease and preparation method thereof

Country Status (1)

Country Link
CN (1) CN115786025B (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101575548A (en) * 2009-06-11 2009-11-11 杭州得润宝油脂有限公司 Lubricating grease special for constant-speed universal joint and preparing method thereof
JP2020083994A (en) * 2018-11-21 2020-06-04 協同油脂株式会社 Grease composition for tapered roller bearing

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101575548A (en) * 2009-06-11 2009-11-11 杭州得润宝油脂有限公司 Lubricating grease special for constant-speed universal joint and preparing method thereof
JP2020083994A (en) * 2018-11-21 2020-06-04 協同油脂株式会社 Grease composition for tapered roller bearing

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张俊杰: "润滑脂的发展及技术现状", 化工管理, no. 31, 1 November 2017 (2017-11-01), pages 64 - 65 *

Also Published As

Publication number Publication date
CN115786025B (en) 2024-04-12

Similar Documents

Publication Publication Date Title
JP5826626B2 (en) Grease composition
EP2540813B1 (en) Grease composition for hub unit bearing equipped with angular contact ball bearing, and hub unit bearing
EP2935539B1 (en) Grease composition
EP2785821B1 (en) Grease composition
JP5604061B2 (en) Grease composition
CN112521997B (en) Lubricating grease composition for metallurgical sintering machine and preparation method thereof
CN111892984B (en) Heavy-duty bearing lubricating grease composition and preparation method thereof
CN105331426A (en) Anti-rust extreme pressure lithium lubricating grease composition and preparation method
CN106433864B (en) A kind of High-temperature-respolent polent pressure grease and preparation method thereof
CN111253997A (en) Composite thickening type polyurea lubricating grease composition and preparation method thereof
CN113512453B (en) Electric automobile hub bearing lubricating grease composition and preparation method thereof
JP5756587B2 (en) Grease composition for angular ball bearing and angular ball bearing using the same
CN106147941B (en) A kind of composite polyurea lubricating grease and preparation method thereof
CN115786025B (en) Organic urea calcium lithium lubricating grease and preparation method thereof
CN108841430A (en) A kind of compound urea aluminium-base grease composition and preparation method
CN107384558B (en) Lubricating grease with intercalation type layered magnesium phosphate as solid lubricating additive and preparation method thereof
CN111718773A (en) Polyurea thickening agent, lubricating grease prepared from polyurea thickening agent and preparation method of lubricating grease
CN112375607B (en) Tetraurea lubricating grease composition and preparation method thereof
CN114426898B (en) Lubricating grease compound additive and lubricating grease composition prepared from same
WO2013017528A1 (en) Grease composition
JP2014108997A (en) Grease composition and rolling bearing
CN113862063A (en) Lubricating grease composition and preparation method and application thereof
CN117448061A (en) Lubricating grease composition for sintering machine and preparation method thereof
CN117801865A (en) Lithium-based lubricating grease composition and application method thereof
JP2014177651A (en) Grease composition

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant